Halogen treatment of oil shale



Sept. 4, 1928. 1,682,743 G. EGLoFF HALOGEN TREATMENT 0F OILl SHALE Original Filed Jan. 14. 1921 @4M Mw- Patented Sept. 4, 19248.

FICE.

dnsrlfv EeLoEF, or INDEPENDENCE, Kansas,

Ucrs COMPANY, or carence, ILLINoIs, a

ASSIGNOR TO UNIERSAL OIL PR01)- CO'RPORATION 0F SOUTH DAKOTA.

HALOGEN TREATMENT OIL SHALE.

Application led January 14, 1921, Serial No. 437,138. Renewed Hay 17, 1927.

This invention relates to improvements in' the halogen treatment of oil shale and refers more particularly to a process and apparatus 'for the treatment of oil shales with they halogen element and internal combustion by means of a rotating still.

I have found that chlorine in the presence of combustion gases limpingin'g upon oil shale kforms chlorides of the metals as for lo instance aluminum chloride. This aluminum chloride generated 'in situ generates or reacts with the products of thev kerogen content of the shale so that the shale oil produced in the presence of the chlorides of the l5 metal yields a light oil content which upon redistillation is a practically refined product suitable for marketing commercially.

The single fi re in the drawing is a vierir partly in side e evation and partly in vertical 20 cross section, of my improved apparatus for carrying out the above process.

Referring in detail to the drawmg, 1 designates a rotatin still in which a burner 1s set.y 3 is an oil s ale hopper, said shale bemg 25 passed into the still 1 through control valve 4 by means of' pi e 5. 6 is a gear around vstill 1, supported y pinion gears 7, which gearing is operated by motor 8 and gear 9. 10 is a vapor line ofthe rotatlng still 1, con- 30 nected to water condenser 11 set in box 12, coil 11 being 'connected to receiver 1 3 by means of pipe 14. The receiver 13 has l1qu1d drawoii" pipe 15 and control valve 16. To th`e upper portion of receiver 13, a pressure a5 gauge 17 is attached, and also an uncondensable gas pipe 18 having control valve 19 attached thereto. The chlorine gas is fed into the system under pressure by means of p1pe 20 and control valve 21, through the perforated pipe 22, set within still 1. 23 is a packing gland to make the system tight. 24 1s a spent shale drawoii pipe having valve 25 attached thereto. The ends 26 and 27 are maintained stationary while the body of the still 28 rotates in the sealed joints 29.

One mode of operation of this process is to charge hopper 3 with the shale to be treated and feeding in said shale through control valve through pipe 5 into still 1. After still "0 1 has been charged with shale, burner 2 is ignited and depending on the shale under treatment, a mellow or a harsh heat may be 1mpinged on the shale while simultaneously chlorine gas is fed intol the system by means of perforated pipe 22. The chlorine reacts in part with the mineral matter the shale, forming chloridesof metal and simultaneously from thls shale,V4 the kerogen content is produced. The volatile aluminum chloridey reacts with the generated hydrocarbon vapors from the kerogen content ofthe shale, passmg out of the still 1 through pi e 10 and is collected in receiver 13. It may e neces,- sary to lnsert in the vapor line a trap to collect the aluminum chloride as a sol-id in said trap. I have found that thealuminum chloride forms addition compounds with some of the hydrocarbons generated in the kerogen and this gives a two-layer system in the receiver. However, this 1s not always the case as 1t depends largely on the type of shale which is being processed. When chlorine gas is used, chloride derivatives of the h dro carbons are formed in addition to the a uminum chloride. These chloride derivatives have their specific commercial use. The hydrocarbon liquid which contains phenolic and nitrogen base compounds when formed in the presence of chlorine yield upon redistillation, gasoline motor fuel, waxes and lubricating oils. The internal temperature impinging on the oil shale in the presence of chlorine may range from 1600 to 2000 degrees or I may use such'dilute combustion gases that an internal temperature may be maintained as low as 600 degrees F., in the presence of chlorine or another halogen.

Aluminum chloride and oil are largely settled out" by gravity in the receiver and they may be separately collected in a receiver having drawoii' pipe 15 and throttle valve 16 as shown. In the event the oil shale contains any substantial amount of water, the aluminum chloride is hydrolyzed forming a jell such as aluminum hydroxide or if the temperature is suiiicientlv high, the aluminum hydroxide is converted into aluminum oxide.

I claim as my invention:

1. A process of treating oil shale having an aluminum content, consisting in intro- 10u ducing the shale to a still, in maintaining the shale in a constant state of motion while in said still by a rotary movement of the still, iny subjecting the shale to a distillation heat by directly impinging thereon the heating gases, 10o and in introducing to the still during the distillation of the shale chlorine gas to unite'the aluminum content of the shale to form alumi num chloride.

2. A process "for distilling oil shale, hav- 11o ducing a supply of said shale to a rotating still to be maintained ina state of motion while therein2 in introducing directly into' the still chlorine gas, in subjecting the oil to a distillation heat in the presence of chlorine gas to distill the oil contents of the `shale and unite the chlorine as with the aluminum content of the. oil siale to form aluminum chloride.

3. A process for distilling carbonaceous substances having an aluminum and an oil content comprising introducing such substances to a still, rotating the still to maintain the substances in a state of motion, introducing directly to the still chlorine gas, subjecting the substances and chlorine gas to heat sulcient to 4distill the oil content of the carbonaceous substancesv and unite the chlorine gas with the laluminum contentof thesubstances to form aluminum chloride.

4. A process for treating a carbonaceous.

Asubstance having an aluminum content comprising introducin the'substance to a still,

Y maintaining the su stance in a constant state of motion while in the'stll by rotary movement of the still, subjectng'the substance to a distillation heat by directly impinginv thereon heating ases, introducing to the sti during the disti lation of theV carbonaceous substance chlorine gas to unite with the` aluminum content ofthe substance and form aluminum chloride.

GUs'rAv iisefLoFF.I 

